HuagongsheHuagongshe Chemistry Print Report · For research reference only
Iodine → HCID 178506571, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Iodine | HCID 807 | — |
| Reactant | Potassium Hydroxide | HCID 14797 | — |
| Reactant | 1H-Thieno[3,2-c]pyrazole | HCID 21915429 | — |
| Reactant | Sodium Bisulfite | HCID 23665763 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | HCID 178506571 | HCID 178506571 | 60.5% |
Reaction Steps
To a solution of 1H-thieno[3,2-c]pyrazole (160 mg, 1.29 mmol) and iodine (490 mg, 1.94 mmol) in dimethyl formamide (5 mL) is added potassium hydroxide (220 mg, 3.87 mmol). The mixture is stirred at room temperature for 30 minutes. A solution of sodium bisulfite (200 mg) in water (2 mL) is then added. It is extracted twice with diethyl ether. The combined organic layers are dried over magnesium sulfate and concentrated. The residue is chromatographed (n-heptane-ethyl acetate, 90:100) to afford 195 mg (60%) of 3-iodo-1H-thieno[3,2-c]pyrazole as a beige powder. LC/MS: RT=2.50 minutes, 250.90 m/e (M+1).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07928231B2 |
| Source dataset | uspto-grants-2011_04 |
| ORD ID | ord-906751fb46864f43b3924914090f2381 |
| Source note | uspto-grants-2011_04 |